CN1103560C - Method for producing powdery seasonings - Google Patents
Method for producing powdery seasonings Download PDFInfo
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- CN1103560C CN1103560C CN96105593A CN96105593A CN1103560C CN 1103560 C CN1103560 C CN 1103560C CN 96105593 A CN96105593 A CN 96105593A CN 96105593 A CN96105593 A CN 96105593A CN 1103560 C CN1103560 C CN 1103560C
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/50—Soya sauce
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/14—Dried spices
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Abstract
A method for producing powdery seasoning with constant quality, with no occurrence of coagulation under storage. The method comprises culturing koji mold in heated and expanded defatted soybean, maintaining a dispersion of the resulting culture in a sodium chloride solution under enzymatically active conditions, separately collecting a liquid dispersion medium from the enzymatic reaction product, adding a liquid seasoning to the liquid dispersion medium, and spray drying the resulting mixture.
Description
The present invention relates to a kind of method of producing powdery seasonings, particularly relate to a kind of method of producing powdery seasonings such as powdery soy sauce.
According to the diversified demand of dietetic life, in field of food, developed instant food a large amount of and that flavoring for mixture is edible.Used flavoring major part is with the form production and the processing of powdery in the instant food, and therefore, in quite long one period from produce consumer's hand, powdery seasonings may be stored under the unsuitable condition, for example high temperature, high humidity and excessive the exposure.
Usually when the powdery seasonings production and supply, to consider the unfavorable conditions that these are potential.But the whole unfavorable conditions that can not look to these flavorings to expose all are tending towards favourable.Because preventing unfavorable conditions to make the possibility of its appearance reduce to extremely low measure will finally make production cost obviously rise, this is unpractical certainly.
Powdery seasonings is all or part of to be powdery or granular.The powdery of per unit weight or particulate matter have bigger surface area.Because powdery seasonings also contains hygroscopicity composition such as sodium chloride, thus disadvantageously these independently powdered granule interconnect and form the piece easily condense.
The coagulation of powdery seasonings is brought consequence inferior, the value of grievous injury commodity.Before and after condensing, the mouthfeel of powdery seasonings or local flavor will finally cause destroying.
As the conventional method that prevents that powdery seasonings from condensing, known a kind of method comprises adding and sneaking in dry state and is tending towards hydrophobic edible material from soybeans, i.e. oxidized starch, finished starch such as phosphorylated starch, dextrin, naturally occurring glue such as arabia gum or protein such as gelatin.The some of them method has been used for reality, and for example a kind of method that discloses among the Japanese patent unexamined publication number JP-A-64-039977 is to add dextrin to condense to prevent ＂ powdery soy sauce ＂.
But following problem values must be noted when taking to prevent measure that powdery seasonings condenses according to these known methods.
That is exactly, and mixes if become hydrophobic edible material from soybeans and powdery seasonings etc. under the dry state, and these materials must add with quite high concentration, and for example the acid anhydride by them approximately is 10-30%wt.
These materials never should destroy the basic mouthfeel and the local flavor of flavoring.For this reason, these materials should be selected from dried as far as possible those materials of tasteless mouthfeel.
When material tasteless or that mouthfeel is dried as far as possible is added to when reaching the effect that this material under the ultimate density can realize preventing condensing in the powdery seasonings, powdery taste substance result is also diluted, has therefore reduced the mouthfeel and the local flavor of UD powdery seasonings.In other words, may reduce the effect of powdery seasonings significantly.
And, add the appearance change that can be observed powdery seasonings behind these materials, promptly non-natural sensation.
Add when preventing to produce the material that condenses, need additional treatment step, for example further add sodium chloride or salt, purpose is the damage that overcomes with correcting unit dosage flavoring mouthfeel and local flavor.
Compare with powdery seasonings itself, it is very expensive that great majority are inclined to hydrophobic edible material from soybeans in dry state.So, by add powdery seasonings that these material productions have the coagulation of preventing can be much raising production cost with avoiding, for this reason, the raising of production cost limited add the scope of selective material.
In the powdery seasonings production process, in dry run, be to carry out spray-drying mostly particularly.But when with the raw material liquid flavoring for mixture, the dry state hydrophobic substance forms the solution of thickness, is unfavorable for operation.In addition specifically, hydrophobic substance in the incipient stage dry state so is difficult to the raw material liquid flavoring miscible, so that need the extra work of some troubles such as special whipping step or heating, purpose in order to make these materials energy and even mixing of liquid condiment is to prevent to form any coagulation or piece.Like this, whole process will be very complicated.And the adhesion that takes place on the spray dryer inwall makes the output of product lower, and the quiet run that will block drier.In addition, because raw material is may part overheated between dry period, also can produce disadvantageous the situation for example decomposition or the sex change of sense of taste composition or flavor ingredient.
It is also noted that some dry states are inclined to hydrophobic edible material from soybeans can produce the accessory substance that products obtained therefrom is had ＂ brown stain ＂ reaction when dry run or storage.
As mentioned above, comprise that with regard to the known method that prevents that powdery seasonings from condensing adding dry state is inclined to hydrophobic edible material from soybeans, also fails to overcome significantly those problems at present.For addressing these problems, conventional method has expended a large amount of living technical forces that has, but does not find desirable way as yet.
The purpose of this invention is to provide the method for under stable state, extensive, low-cost situation, producing high-quality powdery seasonings, thereby overcome the problems referred to above, and definitely prevented from powdery seasonings, to occur condensing.
A kind of selective method that instead comprises the conventional method of adding those edible material from soybeans the invention provides a kind of reality and the method for effectively producing powdery seasonings, and this flavoring becomes hydrophobicity in dry state as mentioned above.Prevent that by the powdery seasonings of the present invention's acquisition is also suitable the conventional powdered flavoring from condensing or a kind of additive of sex change.
According to the present invention, these dry states become hydrophobic powdery seasonings and are made up of the hydrolysate that mould aspergillus of Huang and vegetable protein reaction produce.
Especially, the method that the most preferred embodiment of the present invention provides a kind of production to contain the powdery seasonings of hydrolysate, this hydrolysate are to be produced by the yellow mould aspergillus reaction of defatted soybean itself and soy sauce brewing in the solid medium of mainly being made up of defatted soybean.
In fact the method according to this invention comprises the suitable step that mixture that hydrolysate and the sincere flavoring of liquid by defatted soybean of desiring powder process are formed carries out spray-drying and powder process.
The present invention relates to produce the method for powdery seasonings, what this powdery seasonings contained higher level is flavor amino acid, low molecular peptide, does not occur condensing or sex change keeping good mouthfeel and local flavor after the production or even under long-term disadvantageous storage requirement.Therefore, powdery seasonings of the present invention is applicable to a lot of places, for example as the flavoring of the instant food of shelf long shelf-life.
According to an aspect of the present invention, the method for production powdery seasonings comprises: the step that forms expanded soybean by quick step-down heating and expanded defatted soybean; In the expanded soybean that obtains through above-mentioned expanded step, cultivate yellow mould aspergillus; Under the enzymatic activity condition and in sodium chloride solution, keep culture dispersion liquid from above-mentioned incubation step with the form of aqueous dispersion; Collect liquid dispersion medium respectively in the product that from above-mentioned maintenance step, produces; By on this collects and to add liquid condiment in the liquid dispersion medium that step obtains and obtain a kind of mixture; Spray-drying mixt.
Among the present invention, the powdery seasonings product comprises the material of often classifying with flavoring, the soy sauce of that for example do and soy sauce, ＂ miso ＂ dried and powdery (Miso) or brew powdery, dried and worcester sauce powdery, crystal or graininess ＂ delicious seasoning product ＂, salt crystal or particle, various raw material flavouring, the brew fish sauce of the yeast extract of powdery, powdery for example, various fine spices such as ＂ pepper mixed powder ＂ and ' pimiento mixed powder ＂ etc.
In addition, the various edible instant soup blends of adding hot water that need also can be by the high quelite product classification of powdery of the present invention, for example: ＂ instant soluble soybean Miso Soup ＂, the instant clear soup ＂ of ＂, soup such as the instant potage ＂ of ＂, the instant French thick soup ＂ of ＂ that various adding hot water are edible, various ＂ sprinkling food ＂ such as ＂ pine fillet (katsuo-flake) sprinkling powder ＂, ＂ marine alga-tea sprinkling powder ＂, the China bowl noodle soup material ＂ that the powdery seasonings relevant with various instant foods such as instant soup blend ＂, the ＂ of the packed Chinese noodle of ＂ are instant.
Embodiment preferred according to the present invention, this method is undertaken by the process that may further comprise the steps: cultivate yellow mould aspergillus in expanded soybean; Under the enzymatic activity condition and in sodium chloride solution, keep bent culture dispersion liquid from above-mentioned incubation step with the form of aqueous dispersion; From the product of gained, collect liquid dispersion medium respectively; The mixture of spray-drying liq decentralized medium and liquid quelite.
Because what cultivate in expanded soybean is yellow mould aspergillus, so suitable with the yellow mould aspergillus of soy sauce brewing.Yellow mould aspergillus can be cultivated in the solid medium by expanded soybean system, this expanded soybean is to utilize extruder that NSI (nitrogen soluble index) is equal to or greater than 30 defatted soybean to heat with expanded and make, make puffing process after final antigen titration degree be equal to or less than 3; Add water to last water content in the above-mentioned soybean subsequently and be equal to or less than 40wt%, with the preparation solid medium for being equal to or greater than 30wt%-.
As the defatted soybean of raw material, suitable is through the defatted soybean cake of solvent extraction or the soya-bean cake product that grinds.But, should avoid defatted soybean with the serious sex change of protein.In other words, NSI is equal to or greater than 30 defatted soybean or soy meal and is suitable as raw material.
NSI, the definition of nitrogen soluble index is: the percentage (%) that is determined at the total nitrogen content of the total nitrogen content of the sample of water-soluble extract under the stirring at room and sample with Kjeldahl method for nitrogen determination (Kjeldahl method).This index is the index of representative sample protein denaturation degree.
In order to heat and expanded defatted soybean, preferably utilize method by extruder, various types of extruders, promptly single shaft or twin shaft all can use satisfactorily.
Before the extrusion operation, preferably add the about 10wt%-30wt% that adds water to raw material defatted soybean water content.After so adjusting water content, defatted soybean heats by extruder under pressurized conditions, so, from soybean, discharge steam by quick step-down and come expanded soybean.
In the extrusion operation, should control and regulate the operating condition of extrusion equipment, make heating and expansion process after the antigen titration degree of defatted soybean be equal to or less than 3.
Utilize the antigen titration degree of passive state red blood cell condensation response analysis expanded soybean by the calf antiserum of dilution.The minimum dilution value that red blood cell condensation takes place should be that the logarithm at the end is represented with 2, is called ＂ titer ＂.
In expanded soybean, add water to the end water content be 30wt%-40wt%.
Definite scope of adding the water yield is so that the growth of the sort of quyi of inoculation reaches optimum state.Be lower than this scope, bent poor growth; Be higher than this scope, because excessive water is greater than the water retention of expanded soybean; Bent growth is suppressed.Germ contamination is finally facilitated in overflowing of water.As the yellow mould aspergillus of soy sauce brewing, the soy sauce brewing song that preferential selection mainly is made up of Aspergillus sojae (AspergillusSojae).
As the seed mould of soy sauce brewing song, can use the inoculum of the yellow mould of soy sauce brewing that is purchased.For example, useful commercial ＂ Usumurasaki ＂ by name (buying) from the KABUSHIKI KAISHA HIGUCHI MATSUNOSUKE SHOTEN of Japan.
If desired, can isolate the yellow mould aspergillus of a kind of new soy sauce brewing, regulate its activity, then as inoculum.
The conventional method of soy sauce brewing and condition are applicable to the method and the condition of cultivating the yellow mould aspergillus of soy sauce brewing.
For obtaining aforesaid product or hydrolysate, bent culture should be equal to or less than among the 15wt% under the enzymatic activity condition and at concentration of sodium chloride solution and keep 300 hours with the aqueous dispersion form, up to formaldehyde type nitrogen account for the nitrogen total amount 50% or more.
Should be equal to or less than at concentration of sodium chloride solution and keep bent culture under the 15wt%.The concentration of sodium chloride solution is higher than 15tw%, and following problem may take place: because the reduction of enzymatic activity, the amino acid that can produce tempting taste and the low molecular peptide amount that are contained in the product reduce; The sodium chloride of high concentration can pollute the powdery seasonings product; Or produce strong fermentative smell.
The concentration of preferred sodium chloride solution should be lower than above-mentioned concentration range, for example 3wt%-5wt% particularly.In lower like this concentration range, germ contamination may occur, but the appropriate bacteriostatic agent such as the existence of ethanol and ethyl acetate can suppress germ contamination.
Reaction in the sodium chloride solution continues 300 hours, up to formaldehyde type nitrogen reach contained total nitrogen in the reactive material 50% or more.
Long-time reaction surpasses 300 hours, can produce the unwelcome macromolecule peptide accessory substance that has bitter taste and harsh feeling.Be lower than 50% if formaldehyde type nitrogen accounts for nitrogen pool, then be not enough to produce amino acid and low molecular peptide that tempting taste can be provided.
Measure total nitrogen by known Kjeldahl method for nitrogen determination.Can measure formaldehyde type nitrogen by analyzing formaldehyde, be included in amino acid whose amino and formalin reaction in the sample under the neutral PH, with the hydrogen ion of aqueous slkali titration from amino release.
Bent culture should keep in sodium chloride solution under the enzymatic activity condition.Particularly, culture should keep PH1.5～PH6.5,25 ℃～40 ℃ of temperature.In such scope, it is maximum that bent hydrolytic enzyme activities, particularly proteinase activity reaches.In the above range, the maximum activity of bent hydrolase depends on the kind of yellow mould aspergillus or isolated strains and changes, can preferably pre-determine the particular range that used aspergillus strain presents its peak activity like this.
The product that keeps under the enzymatic activity condition is a water dispersion, contains to come a large amount of amino acid and the low molecular peptide of autospasy ester soybean protein delicious food, and wherein is dispersed with the solid composition of non-degraded.
When the above-mentioned water dispersion that wherein is dispersed with the solid composition was carried out spray-drying, the phenomenon of stopped nozzles can appear once in a while.Therefore, before the spray-drying operation, should remove solid constituent from water dispersion, separation and collection do not contain the liquid dispersion medium of solid composition.
Can without stint utilize the method for any removal solid composition or equipment to collect liquid dispersion medium.For example, can use continuously the centrifuge of racing not, intermittently compression filter and adverse current diffusion separator.
As an example, be used for liquid quelite of the present invention and comprise that soy sauce, squeezing soyabean sauce disperse thing, worcester sauce, savoury flavouring, sodium chloride solution, yeast extract solution, sake-cake extract, brew fish sauce, various fine spices dispersion things such as dispergated pepper powder, dispergated Paprika, the material solution of soy sauce instant soups, the material solution of instant clear soup, the material solution of instant potage, the material solution of instant thick soup, the material solution of fast food Chinese noodle soup stock etc.
In aforesaid those liquid quelites, soy sauce is particular importance and proper raw material.
But use any soy sauce as the liquid soy sauce without stint.Particularly available for example dark type (koikuchi) soy sauce, light color (usukuchi) soy sauce, soybean (tamari) soy sauce, sauce, white (shiro) soy sauce and life (draft) soy sauce again.
What ratio liquid dispersion medium and liquid quelite can take over is mixed mutually and has no particular limits, but, because liquid dispersion medium also tool is the flavor effect, so should determine the mixing ratio of liquid dispersion medium and liquid quelite, the main taste of liquid quelite can not be subjected to heavy damage like this.In addition, consider the taste of the high quelite product of powdery and calculate its concentration, should determine the mixing ratio of this decentralized medium of liquid and liquid quelite.
For example, can utilize common making soy sauce as the raw material of liquid quelite, the weight that the preferred liquid decentralized medium is sneaked into soy sauce is that the total nitrogen in about 0.25～3.0 times or the liquid dispersion medium of soy sauce weight is about 0.4～6.0 of a total nitrogen in the soy sauce.
Be the mixture of spray-drying liq decentralized medium and liquid quelite, can use any method and apparatus by without stint.
For example, can use the drier of constricting nozzle type spray dryer, twin-jet nozzle spray dryer, dish-like spray dryer and spray-drying and granulation.
At spray-drying process, should avoid smell (local flavor) to disappear, but other condition of operation is not particularly limited.For example, available general spray-drying condition is 80-100 ℃ as predetermined air exhaust temperature.
Should note avoiding the part sometimes of raw material liq decentralized medium and liquid quelite overheated.
The overheated ＂ coking ＂ that causes in the equipment of the part of raw material, this causes product yield to descend, and comprises that also the operating efficiency of equipment reduces, and is difficult to cleaning equipment after the attended operation.And, the ＂ brown stain material ＂ apparent damage that produces by ＂ coking ＂ the taste and the local flavor of powdery seasonings.In addition, under storage requirement, these materials can be facilitated the infringement of product colour.
Distinguish the flavor of amino acid and the low molecular peptide of being that contains more amount by the sticking shape flavoring of production method preparation of the present invention.Even under disadvantageous storage requirement, powdery seasonings of the present invention can keep good taste and local flavor and cohesion or sex change do not occur in harsh postpartum for a long time.Therefore, powdery seasonings of the present invention is suitable for the flavoring of the instant food of making the shelf long shelf-life.So this flavoring is applicable to a lot of fields.
The present invention is existing to be described in detail with embodiment.Should note the invention is not restricted to these embodiment.
Embodiment 11A) heating of defatted soybean and expanded:
Defatted soybean (100kg; NSI=60, ＂ KOJIMAME ＂ are made by Japanese TOYO OIL MILL KABUSHIKI KAISHA as name of product) crushing, be placed in the container, add running water (40L) subsequently.The soybean that adds behind the water feeds in the single shaft extruder immediately, and this extruder name of product is ＂ X-150/55 ＂ (being made by WENGER company), and it is the mould of 6mm that the squit hole diameter is installed.Regulate in the extruder cylindrical shell temperature to 150 ℃, the required time by cylindrical shell is 45-55 second, and pressing in the operation middle cylinder body is 8-15kg/cm
2Defatted soybean is heated continuously by cylindrical shell the time and is pressurizeed; Form expanded soybean by quick step-down from the cylindrical shell ejection at outlet opening.1B) in the expanded soybean that obtains by operation 1A, cultivate yellow mould aspergillus:
Obtain the expanded soybean that total amount is 138kg from operation 1A.The moisture of expanded soybean is 28%.Prepare five expanded soybean material groups, every amount is 1.22kg, is cooled to 30 ℃.Then, cultivate yellow mould aspergillus with every expanded soybean material group as follows.
At first, by adjust the water content to 35% of every expanded soybean from nozzles spray 318ml hot water (40 ℃).Then, 1g soy sauce brewing sort of quyi culture is a ＂ Usumurasaki ＂ (ProductName, can buy from Japanese KABUSHIKI KAISHA HIGUCHI MATSUNOSUKE SHOTEN) and the mixing of 1g wheat flour, sow the surface at every expanded soybean equably, every expanded soybean places bent incubator separately.Each case in five casees is carried out 35 ℃ of fermentations 45 hours, every 8 hours with artificial manual mode stir culture thing, stopped bent the cultivation at 45 hours.1C) under the enzymatic activity condition, in sodium chloride solution, keep culture dispersion from operation 1B:
Get five bent cultures from different incubators, every heavy 1.41kg.Every bent culture is soaked into different concentrations of sodium chloride solution (2.4L) also mixes with it to form the culture aqueous dispersion, this dispersion remains in this solution at 30 ℃ and reaches preset time, shown in Table A.
Table A
Concentration (wt%) retention time (hr) example-1 15 300 example-2 15 300 example-3 10 300 example-4 12 170 examples-5 15 170
When the maintenance phase finishes,, from routine 1-5, obtain the product of five kinds of samples of 3.94kg respectively by the hydrolysis of soybean protein, i.e. ＂ sauce wine with dregs ＂ (＂ Moromi ＂) or brewage slurry, the sodium chloride content scope is 7.0～9.5% in these samples.1D) from the product that operation 1C produces, collect liquid dispersion medium:
5 kinds of samples that utilize filter press to squeeze respectively to be obtained by operation 1C separate to carry out solid-liquid, and the filtered fluid that is not had solid thus substantially is a liquid dispersion medium, is respectively 2,500ml.1E) mixing material flavoring and the filtered fluid that is obtained by operation 1D or hydrolysising product solution are to form mixture:
The sample filtering liquid that obtains of reaction is that total nitrogen concentration is that the hydrolysising product solution of 2.5g/dl is light color (Usukuchi) soy sauce (being made by Japanese HIGASHIMARU SOY SAUCE KABUSHIKI KAISHA) of 1.2g/dl with the total nitrogen concentration that is purchased in operation 1D example-1, mixing ratio is 3: 1 (routine A1), 1: 1 (routine B1) or 1: 3 (routine C1).The total nitrogen ratio of these mixtures is 1: 0.7 (A1), 1: 2.1 (B1) and 1: 6.2 (C1).1F) the mixture that obtains by operation 1E of spray-drying:
To these mixture solutions, every part of basic 1L carries out spray-drying, use be jet pipe type spray dryer, model ON-20 (making) by Japanese KABUSHIKI KAISHA OKAWARASEISAKUSHO.In operating process, regulate the air exhaust temperature to 95 ℃ of drier blast pipe, make three kinds of powdery soy sauce test specimen A1, B1 and C1 (Sample A 1, B1 and C1), be respectively 72g (A1), 70g (B1) and 75g (C1).The water content of sample is 8.2% (A1), 7.7% (B1) and 6.0% (C1).
Simultaneously, under identical condition, only light color (usukuchi) soy sauce spray-drying is prepared powdery soy sauce control sample Ac1 (contrast Ac1); Add dextrin (making) preparation powdery soy sauce control sample Bc1 (contrast Bc1) by Japanese SANWA DENPUNKABUSHIKI KAISHA, replace hydrolysising product solution, the dry of its cereal (awakuchi) soy sauce is 30wt%, prepares dispersion and spray-drying dispersion liquid under the same conditions.Here, the glucose equivalent (D.E.) of dextrin is 6～8 among the contrast Bc1.1G) producing powdery soy sauce process evaluation viscosity:
Respectively to material solution spray-drying 1 hour or the long-time operation as much as possible of note sample A1, B1 and C1 and contrast Ac1 and Bc1, under macroscopic view, estimate the sample viscosity in the drying tower inwall and pipe fitting in the spray dryer.The standard of estimating is divided into the sticking anything but ＂ (◎) of 4 kinds of ＂, the sticking slightly ＂ (zero) of ＂, and very sticking ＂ of ＂ (△) and ＂ can't operate ＂ (X) owing to sticking.Table 1 shows evaluation result.
Viscosity sample (material solution) viscosity during table 1 powdery soy sauce is produced is soy sauce to Ac1 (Usukuchi ss) △ in the same old way to the numeral in Bc1 (ss+ dextrin) zero Sample A 1 (3: 1) △ sample B 11 (1: 1) zero sample C1 (1: 3) the ◎ round parentheses in the same old way: hydrolysate (weight ratio), ＂ ss ＂ refers to soy sauce.
As shown in table 1, sample B 1 and C1 promptly add 50% or the sample of logical many hydrolysising product solutions in, the viscosity number to Bc1 in the same old way of observing viscosity number and interpolation dextrin is the same or lower.On the contrary, observed the tangible viscosity of contrast Ac1 at about 30 minutes, therefore, operation can not be carried out continuously again.1H) determine the moisture content retention of powdery soy sauce:
After operation 1F spray-drying, 5 kinds of samples are pattern A1, B1 and C1 and are that the thermostatic drier of metal wire heater (is the water retention that ＂ Circulation Oven ＂ (being made by Japanese MITAMURA RIKEN KABUSHIKIKAISHA) detects them immediately to Ac1 and Bc1 in the same old way by the thermal treatment zone altogether.These samples make it leave standstill in an airtight container then and are cooled to room temperature being to keep 4 hours under 105 ℃ and the environmental pressure in sample temperature in the drier.Table 2 has shown that the dry back loss in weight accounts for the percentage of original weight.
10.0 couples of moisture content retention sample water retention (%) the contrast Ac1 (Usukuchi ss) that table 2 follows the powdery soy sample after the spray-drying closely the number in Bc1 (ss+ dextrin) 7.8 Sample A 1 (3: 1) 8.2 sample B 1 (1: 1) 7.7 sample C1 (1: 3) 6.0 round parentheses in the same old way are soy sauce: hydrolysate (weight ratio), ＂ ss ＂ refers to soy sauce.
As shown in table 2, to observe and only contain light color (Usukuchi) soy sauce Ac1 is in the same old way compared, the Sample A 1, B1 and the C1 degree of drying that add hydrolysate are obviously higher; The degree of drying of also observing these samples with add the identical or than its height of dextrin to Bc1 in the same old way.And show that it is to be directly proportional that degree of drying approximately adds hydrolysate with institute.1I) powdery soy sauce water retention is over time:
Whole 5 samples are pattern A1, B1 and C1 and Ac1 and Bc1 in the same old way are stored in relative humidity is 0 day (after following spray-drying closely) in 33 ± 2% the environment, 3 days, 7 days or 17 days.Detect their water retention.Utilize the method and apparatus identical with operation 1G.The water retention variation of each storage period is listed in the table 3.
Table 3 powdery soy sample water retention over time (%) sample storage period (my god)
Numeral in 037 17 contrast Ac1 (Usukuchi ss), 10.0 11.8 11.9 12.0 contrast Bc1 (ss+ dextrin), 7.8 9.5 10.3 10.2 Sample A 1 (3: 1), 8.2 10.7 11.0 11.0 sample B 1 (1: 1), 7.7 9.3 9.7 9.7 sample C1 (1: 3), 6.0 9.2 9.5 9.5 round parentheses is soy sauce: hydrolysate (weight ratio), ＂ ss ＂ refers to soy sauce.
As shown in table 3, observe: with only contain light color (Usukuchi) soy sauce Ac1 is in the same old way compared, Sample A 1, B1 and the C1 that adds hydrolysate begins time to 17 immediately and day maintains high drying regime after drying, the degree of drying to Bc1 in the same old way of Sample A 1, B1 and C1 and interpolation dextrin is identical or more higher than it.And, observe the water retention order of magnitude of measuring immediately after the spray-drying and do not change in whole storage period, any sample does not have significant change at 3 days and after this water retention, and this shows and follows lower water retention after the spray-drying closely, if present, can remain to always after.1J) the variation of powdery soy sauce equilibrium humidity in the environment of different humidity:
Whole 5 samples are Sample A 1, B1 and C1 and to Ac1 and Bc1 seasoning in the same old way under constant temperature and damp condition 7 days, and relative humidity is being equal to or less than 10%, 22%, 32%, 42% or 52%, 20 ℃ of identical temperature.Then, measure their water retention.Used method and apparatus is the same with operation 1H's.The equilibrium humidity of each sample of each relative humidity is listed in the table 4.
Variation (%) the sample relative humidity (%) of table 4 equilibrium humidity of powdery soy sample in the different humidity environment
Numeral in＜10 22 32 42 52 contrast Ac1 (Usukuchi ss) 10.2 10.4 11.4 12.2 16.2 contrast Bc1 (ss+ dextrin) 8.0 9.5 9.8 11.5 15.5 Sample A 1 (3: 1) 8.2 9.6 10.4 11.5 15.5 sample B 1 (1: 1) 7.6 9.5 9.6 11.5 15.5 sample C1 (1: 3) 6.5 7.8 8.3 10.0 13.8 round parentheses is soy sauce: hydrolysate (weight ratio), ＂ ss ＂ refers to soy sauce.
As shown in table 4, observe: with only contain light color (Usukuchi) soy sauce Ac1 is in the same old way compared, the Sample A 1, B1 and the C1 that add hydrolysate remain on high drying regime under each relative humidity.Also observe: the degree of drying to Bc1 in the same old way of Sample A 1, B1 and C1 and interpolation dextrin is identical or more higher than it.And observe: measured and follow after the spray-drying water retention order of magnitude under each relative humidity and this value closely and basically afterwards and do not change.Therefore, show under each relative humidity to keep lower moisture content retention, if this value at once water retention after low scope just depends on spray-drying.1K) powdery soy sauce flowability is over time:
Whole 5 samples promptly try A1, B1 and C1 and contrast Ac1 and Bc1 be stored in the Polypropylene Bag of opening 0 day (after the spray-drying at once), 3 days, 7 days, 17 days and 90 days, be 33 ± 2% times in relative humidity.Then, with the naked eye or the variation of under finger tip collision in addition, checking the mobility variations of these powder and wherein occurring condensing.Observe the flowability of each of powdery seasonings storage period.The results are shown in the table 5.In table, symbol zero expression ＂ good fluidity ＂, △ represents that ＂ flips current downflow ＂, and * represents that ＂ heavily bumps current downflow ＂, and * * represents that ＂ splits by force to condense and is difficult for decomposing ＂, and * * * represents that ＂ is very fast and seriously condenses and hygroscopic effect takes place and begin deliquescence ＂.
The flowability of table 5 powdery soy sample over time sample each storage period (my god) state
Numeral in 037 17 90 control sample Ac1 (Usukuchi ss), zero △ * * * * * * control sample Bc1 (ss+ dextrin), 00 △ * * * * * Sample A 1 (3: 1), 000 △ △ sample B 1 (1: 1), 0000 △ sample C1 (1: 3), 00000 round parentheses is soy sauce: hydrolysate (weight ratio), ＂ ss ＂ refers to soy sauce.
As shown in table 5, examination A1, the B1 and the C1 that add hydrolysate keep good flowability for a long time; These samples can't see any condensing substantially when surpassing 90 days.On the contrary, the contrast Ac1 that only contains light color (usukuchi) soy sauce condensed in the time of the 7th day; Ac1 in the same old way was tending towards moisture absorption is the deliquescence state after 90 days.Add dextrin to Bc1 in the same old way 7 days and after condense, at 17 days and be later strong coagulated state.1L) the variation of powdery soy sauce taste and fragrance (local flavor) after storage:
Whole 5 samples, i.e. Sample A 1, B1 and C1 and to be stored in the Polypropylene Bag of opening 0 day for 33 ± 2% times in relative humidity (after the spray-drying at once) or 17 days of Ac1 and Bc1 in the same old way.Then, these samples carry out the sensory evaluation test.Every duplicate samples is dissolved in the water that ion exchange resin treatment crosses, and ultimate density is 1.0wt%/vol%, remains in 25 ℃ then.For sensory evaluation, with a kind of form (or in round table mode) of colloquy sample solution by Testing Team's check gained of 7 member compositions, examination mouthfeel (good to eat with become the flavor degree), local flavor (having or not the smell of burning, flavor of soy sauce degree) and tone (dark or shallow).The conclusion of evaluation result based on everyone is divided into three grades of fine ＂ of ＂ (putting on ◎), and good ＂ of ＂ (putting on zero) and ＂ observe some defective ＂ (putting on △).The results are shown in the table 6 of relevant each evaluation.
Table 6 powdery soy sample is stored the variation of back mouthfeel and local flavor
Storage period: after the spray-drying at once
Storage period: stored back 17 days
| Sample | Sensory test is estimated | |||||
| Mouthfeel | Local flavor | Color | Conclusion | |||
| Delicious taste | Become flavor | The smell of burning | The ss local flavor | Tone | Estimate | |
| Contrast Ac1 (Usukuchi ss) contrast Bc1 (ss+ dextrin) Sample A 1 (3: 1) sample B 1 (1: 1) sample C1 (1: 3) | Dense weak dense dense | Dense weak getting well carefully | Weak a little less than dense the detecting | A little less than dense carefully a little less than | The depth is deeply dark | △ ? ? △ ? ◎ ? ◎ ? ◎ |
| Control sample Ac1 (Usukuchi ss) control sample Bc1 (ss+ dextrin) Sample A 1 (3: 1) sample B 1 (1: 1) sample C1 (1: 3) | Dense weak dense dense | Dense weak getting well carefully | Dense detecting a little less than the nothing | A little less than detecting carefully a little less than | The depth is deeply dark | △ ? ? △ ? ◎ ? ◎ ? △ |
The numeral soy sauce in the round parentheses and the weight ratio of hydrolysate, ＂ ss ＂ refers to soy sauce.
As shown in table 6, in the Sample A 1, B1 and the C1 that add hydrolysate, when storing 17 days, do not observe the destruction of any mouthfeel, local flavor or tone substantially.On the contrary, when storing 17 days, only by light color (usukuchi) soy sauce form to Ac1 in the same old way and add dextrin to observing the destruction of mouthfeel, local flavor and tone among the Bc1 in the same old way.Particularly Ac1 in the same old way is subjected to heavy damage.After the spray-drying at once and after, to Bc1, weak flavor poorer in the same old way than the mouthfeel of other sample; Tone obviously is efflorescence.
Embodiment 22A) preparation of dusty yeast extract:
The yeast extract of paste is ＂ yeast peptone cream ＂ (100g; By Bio-Springer Co., Ltd system) be dissolved in the water (600g) that ion exchange resin treatment crosses, make the dispersion thing.Then, filter out the solid matter that disperses in the thing.Sneak into the identical hydrolysising product solution with embodiment 1 operation 1E in this yeast extract solution, mixing ratio is 3: 1 (routine A2), 1: 1 (routine B2) or 1: 3 (routine C2).These mixture solutions are spray-drying under the condition identical with embodiment 1 operation 1F, makes three kinds of dusty yeast extract Sample A 2, B2 and C2.Here, the nitrogen ratio of mixture solution is 1: 0.7 (routine A2), 1: 2.1 (routine B2) and 1: 6.3 (routine C2) successively.
Under identical condition, the yeast extract solution that a spray-drying is identical, preparation dusty yeast extract control sample Ac2 (to Ac2 in the same old way).Viscosity during 2B) evaluation powder yeast extract is produced:
To Sample A 2, B2, C2 with to the material solution of Ac2 (mixture solution) spray-drying 1 hour in the same old way or the operating time is prolonged, under macroscopic view, the viscosity of those samples in drying tower inwall and the pipe fitting in spray dryer is estimated respectively.As embodiment 1 operation 1G, the evaluation of standard is divided into sticking slightly ＂ (putting on zero), ＂ of four kinds of ＂ sticking anything but ＂ (putting on ◎), ＂ extremely sticking ＂ (putting on △), ＂ can't operate ＂ (putting on X) because of sticking.Table 7 is expressed the result of evaluation.
Viscosity sample (material solution) viscosity during table 7 dusty yeast extract is produced is the weight ratio of yeast extract and hydrolysate to the numeral in Ac2 △ Sample A 2 (3: 1) △ sample B 2 (1: 1) ◎ sample C2 (1: 3) the ◎ round parentheses in the same old way.
As shown in table 7, in sample B 2 and C2, promptly add 50% or the sample of more hydrolysate, do not observe any viscosity substantially.The slight goo that occurs can be removed (peeling off) from inner wall of tower fully through shaking the drying tower outer wall gently.On the contrary, in the time of about 25 minutes, only contain yeast extract to observe bigger viscosity among the Ac2, continued operation more for this reason in the same old way.2C) the moisture content retention of analysis dusty yeast extract:
After following the spray-drying of above-mentioned operation 2A closely, whole four samples are Sample A 2, B2, C2 and Ac2 is in the same old way being utilized their water retention of measurement under the drier identical with embodiment 1 operation 1H, the identical condition.Measuring the water retention is listed in the table 8.
The water retention sample water retention (%) that table 8 follows dusty yeast extract sample after the spray-drying closely is the weight ratio of yeast extract and hydrolysate to the numeral in Ac2 (yeast extract solution) 10.5 Sample A 2 (3: 1) 9.2 sample B 2 (1: 1) 8.0 sample C2 (1: 3) 6.5 round parentheses in the same old way.
As shown in table 8, by yeast extract is formed Ac2 is in the same old way compared, the degree of drying of Sample A 2, B2 and C2 that adds hydrolysate is obviously higher with only.And, observe its degree of drying and approximately be directly proportional with the amount that adds hydrolysate.
Embodiment 33A) preparation powdery sake-cake extract:
The water that the sake-cake of sheet (being made by Mercian Co., Ltd) is crossed with the ion exchange resin treatment that is four times in its weight disperses and suspends in water, fully swelling subsequently.Then, in the suspension of gained, add protease and cellulase (all making) by AmanoPharmaceuticals Co., Ltd.Mixture was retained to 40 ℃ after 30 hours, filtered out the solid matter in the suspension.Add the hydrolysate identical with the operation 1E of embodiment 1 in this pure mellow wine extract solution, making the final weight ratio is 5: 1 (routine A3), 4: 1 (routine B3), 3: 1 (routine C3), 2: 1 (routine D3) or 1: 1 (routine E3).These mixtures of spray-drying under the condition identical with embodiment 1 operation 1F reclaim 5 kinds of powdery sake-cake extract Sample A 3, B3, C3, D3 and E3.Here, the nitrogen ratio in the mixture solution is followed successively by 1: 0.45 (routine A3), 1: 0.57 (routine B3), 1: 0.76 (routine C3), 1: 1.1 (routine D3) and 1: 2.3 (routine E3).
Under identical condition,, be recovered to the sake-cake extract control sample Ac3 (to Ac3 in the same old way) of paste in addition more only to spilling slag extract solution spray drying clearly.Viscosity during 3B) evaluation powdery sake-cake extract is produced:
Respectively to Sample A 3, B3, C3, D3, E3 with to material solution spray-drying 1 hour or the long-time operation as far as possible of Ac3 in the same old way, under macroscopic view, estimate the viscosity of the sample in the drying tower inwall and pipe fitting in the spray dryer.Press the operation 1G of embodiment 1, the evaluation of standard becomes four kinds: sticking slightly ＂ (putting on zero), very sticking ＂ of ＂ (putting on △) of ＂ sticking anything but ＂ (putting on ◎), ＂ and ＂ can't operate ＂ (putting on X) because of sticking.Evaluation result is listed in the table 9.
Numeral in viscosity sample (material solution) viscosity control sample Ac3 (sake-cake extract solution) X Sample A 3 (5: 1) △ sample B 3 (4: 1) zero sample C3 (3: 1) zero sample D3 (2: 1) ◎ sample E3 (1: 1) the ◎ round parentheses during table 9 powdery sake-cake extract is produced is the weight ratio of sake-cake extract solution and hydrolysate.
As shown in table 9, in sample C3, D3 and E3, promptly be equal to or greater than in the sample of 25% hydrolysising product solution in interpolation, do not observe any viscosity; In other words, only observe extremely slight viscosity.On the other hand, begin operation after, only by sake-cake take out the extract solution composition to Ac3 in the same old way at once with regard to toughness.Subsequently, viscosity increases fast up to continued operation again.The result can not produce the product of powdery, can only be recovered to the product of paste.3C) determine the water retention of powdery sake-cake extract:
Utilize the drier identical with embodiment 1 operation 1H, under identical condition, determine the water retention of whole 6 kinds of samples, they be occur after degree sample A3, B3, C3, D3 and E3 and the spray-drying that reclaims at once after the spray-drying among the operation 3A viscosity to Ac3 in the same old way.Measure the water retention.The results are shown in the table 10.
The water retention sample water retention (%) that table 10 follows powdery sake-cake extract after the spray-drying closely is to Ac3 (sake-cake extract) in the same old way
* 1---Sample A 3, (5: 1) 9.5 sample B 3, (4: 1) 8.4 sample C3, (3: 1) 7.5 sample D3, (2: 1) 5.0 sample E3, numeral in (1: 1) 4.5 round parentheses is the weight ratio of sake-cake extract solution and hydrolysate.* 1) paste goo (can not reclaim powder)
As shown in table 10, the contrast Ac3 that does not add additive with only being made up of the sake-cake extract compares, and the degree of drying of Sample A 3, B3, C3, D3 and the E3 of interpolation hydrolysate is obviously higher.And, observe degree of drying and approximately be directly proportional with the amount of added hydrolysate.Also further observe, to tangible ＂ smell of burning ＂ and ＂ brown stain ＂ phenomenon take place among the Ac3 in the same old way.
As mentioned above, advantage of the present invention is: under low-cost, the condition that is suitable for producing in batches, spray-drying can be operated and makes high-quality powdery seasonings in mode stably.Simultaneously, the powdery seasonings of being produced by the inventive method can keep good powdery and not occur condensing or degenerating under abominable storage requirement.Therefore, the flavoring that so obtains can keep good mouthfeel and the local flavor that was had at that time after the spray-drying for a long time.
Claims (7)
1. borrow the method for spray-drying for one kind, be characterised in that said method comprising the steps of by liquid or paste mixture production powdery seasonings:
A) heating also forms expanded soybean through the quick expanded defatted soybean of step-down;
B) in the expanded soybean of step a) gained, cultivate yellow mould aspergillus;
C) under the enzymatic activity condition, be equal to or less than in the sodium chloride solution of 15wt% in concentration, keep reaching 300 hours with the aqueous dispersion form from the dispersion thing of the culture of step b), up to formaldehyde type nitrogen reach wherein contained nitrogen pool 50% or more, the pH scope of wherein said aqueous dispersion is 1.5-6.5, and temperature is 25 ℃-40 ℃.
D) from the product that step c) produces, collect fluid dispersion separately;
E) in the liquid dispersion medium that step d) obtains, add liquid quelite, obtain described mixture by described spray drying process efflorescence.
2. produce the method for powdery seasonings according to claim 1, the water-soluble nitrogen index that is characterised in that the step a) defatted soybean is equal to or greater than 30%, and through the extruder heating while puffing, make last antigen titration degree equal 3 or less than 3, in above-mentioned defatted soybean, add water before the step b), make last water content account for the 30wt%～40wt% of gross weight.
3. produce the method for powdery seasonings according to claim 1, be characterised in that the mould aspergillus of described Huang is the yellow mould aspergillus of soy sauce brewing.
4. produce the method for powdery seasonings according to claim 1, the concentration that is characterised in that sodium chloride solution is 3wt%-5wt%.
5. produce the method for powdery seasonings according to claim 1, be characterised in that sodium chloride solution contains antibacterial substance.
6. produce the method for powdery seasonings according to claim 1, be characterised in that soy sauce is used as liquid quelite.
7. produce the method for powdery seasonings according to claim 6, be characterised in that liquid dispersion medium sneaks in the liquid quelite, the former and liquid quelite weight ratio are 0.25-3.0, and total nitrogen is the 0.4-0.6 of liquid quelite total nitrogen.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP052024/95 | 1995-02-17 | ||
| JP7052024A JPH08214829A (en) | 1995-02-17 | 1995-02-17 | Production of powdery seasoning |
| JP052024/1995 | 1995-02-17 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1135853A CN1135853A (en) | 1996-11-20 |
| CN1103560C true CN1103560C (en) | 2003-03-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96105593A Expired - Fee Related CN1103560C (en) | 1995-02-17 | 1996-02-16 | Method for producing powdery seasonings |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US5980957A (en) |
| EP (1) | EP0727153B1 (en) |
| JP (1) | JPH08214829A (en) |
| CN (1) | CN1103560C (en) |
| DE (1) | DE69611193T2 (en) |
| MY (1) | MY126337A (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3590225B2 (en) * | 1996-12-09 | 2004-11-17 | キッコーマン株式会社 | Seasoning manufacturing method |
| JPWO2004008880A1 (en) * | 2002-07-24 | 2005-11-17 | ピースビーンズ株式会社 | Processed soybean material and manufacturing method thereof |
| JP4525348B2 (en) * | 2002-08-23 | 2010-08-18 | 不二製油株式会社 | Instant food |
| KR100506832B1 (en) * | 2002-12-31 | 2005-08-10 | 주식회사 해찬들 | The Method of Koji Making for Reduced Hotness Gochujang, and The Koji Made by The Method and Gochujang Made by The Koji |
| US7403966B2 (en) * | 2003-12-08 | 2008-07-22 | Freescale Semiconductor, Inc. | Hardware for performing an arithmetic function |
| JP4595332B2 (en) * | 2004-01-27 | 2010-12-08 | キトサン食品工業株式会社 | Shochu dried product and its manufacturing method |
| CN101242746B (en) * | 2005-11-17 | 2012-03-28 | 龟甲万株式会社 | Seed koji for brewing, koji for brewing, brewed foods, and method for producing the same |
| WO2009108769A2 (en) * | 2008-02-27 | 2009-09-03 | Cadbury Adams Usa, Llc | Multi-region confectionery |
| JP5565625B2 (en) * | 2010-08-27 | 2014-08-06 | 学校法人武庫川学院 | Worcester sauce manufacturing method and Worcester sauce obtained thereby |
| CN103371374B (en) * | 2012-04-25 | 2015-01-07 | 味之素株式会社 | Production method of oil-containing meat particle powder and condiment prepared by using method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4449987A (en) * | 1981-10-29 | 1984-05-22 | Avon Products, Inc. | Fragrant insect repellent composition and combustible candle composition containing same |
| CN1092616A (en) * | 1993-04-14 | 1994-09-28 | 长沙市蔬菜科学研究所 | Edible fungus protein series nutritive soy sauce |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA971031A (en) * | 1972-12-11 | 1975-07-15 | Tadanobu Nakadai | Process for manufacturing soy sauce using enzymatic preparation(s) |
| JPS52130996A (en) * | 1976-04-27 | 1977-11-02 | Kikkoman Corp | Malt preparation |
| JPS5733570A (en) * | 1980-08-05 | 1982-02-23 | Yamanaga Shoji Kk | Preparation of new seasoning |
| JPS6019979B2 (en) * | 1980-12-20 | 1985-05-18 | ヤマカ醤油株式会社 | Salt-free flavor seasoning manufacturing method |
| JPS57177669A (en) * | 1981-04-24 | 1982-11-01 | Sato Shokuhin Kogyo Kk | Koji-containing alcoholic seasoning powder and its preparation |
| JPS58212762A (en) * | 1982-06-02 | 1983-12-10 | Kiroku Yazaki | Novel seasoning |
| JPH0611223B2 (en) * | 1985-04-24 | 1994-02-16 | 株式会社ホーネンコーポレーション | Manufacturing method of soy sauce made from defatted soybean |
| US4892746A (en) * | 1987-01-07 | 1990-01-09 | Donida Carlos O | Powdered soybeam extract |
| JPH0675480B2 (en) * | 1990-11-28 | 1994-09-28 | フンドーキン醤油株式会社 | Method for producing unsalted animal-fermented powder seasoning |
| JPH07327631A (en) * | 1994-06-10 | 1995-12-19 | Ajinomoto Co Inc | Production of high-nitrogen seasoning composition |
-
1995
- 1995-02-17 JP JP7052024A patent/JPH08214829A/en active Pending
-
1996
- 1996-02-14 EP EP96301005A patent/EP0727153B1/en not_active Expired - Lifetime
- 1996-02-14 DE DE69611193T patent/DE69611193T2/en not_active Expired - Fee Related
- 1996-02-16 CN CN96105593A patent/CN1103560C/en not_active Expired - Fee Related
- 1996-02-16 MY MYPI96000608A patent/MY126337A/en unknown
- 1996-02-20 US US08/605,551 patent/US5980957A/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4449987A (en) * | 1981-10-29 | 1984-05-22 | Avon Products, Inc. | Fragrant insect repellent composition and combustible candle composition containing same |
| CN1092616A (en) * | 1993-04-14 | 1994-09-28 | 长沙市蔬菜科学研究所 | Edible fungus protein series nutritive soy sauce |
Also Published As
| Publication number | Publication date |
|---|---|
| US5980957A (en) | 1999-11-09 |
| JPH08214829A (en) | 1996-08-27 |
| EP0727153B1 (en) | 2000-12-13 |
| MY126337A (en) | 2006-09-29 |
| EP0727153A3 (en) | 1996-11-06 |
| CN1135853A (en) | 1996-11-20 |
| DE69611193D1 (en) | 2001-01-18 |
| EP0727153A2 (en) | 1996-08-21 |
| DE69611193T2 (en) | 2001-08-02 |
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